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Abd El-Hady D.,King Abdulaziz University | Abd El-Hady D.,Assiut University | Albishri H.M.,King Abdulaziz University | Rengarajan R.,King Abdulaziz University | Watzig H.,Institute of Medicinal and Pharmaceutical Chemistry

Methotrexate (MTX) is widely used for the treatment of many types of cancer. Folinic acid (FNA) and folic acid (FA) were usually simultaneously supplemented with MTX to reduce the side effects of a folate deficiency. This study, for the first time, included on-line sample preconcentration by stacking and sweeping techniques under reduced or enhanced electric conductivity in the sample region using short chain alkyl imidazolium ionic liquids (ILs) as micelle forming agents for analyte focusing. Both analyte focusing by micelle collapse (AFMC) and sweeping-MEKC had been investigated for the comparison of their effectiveness to examine simultaneously MTX, FNA and FA in plasma and urine under physiological conditions. In sweeping-MEKC, the sample solution without micelles was hydrodynamically injected as a long plug into a fused-silica capillary pre-filled with phosphate buffer containing 3.0 mol/L of 1-butyl-3-methylimidazolium bromide (BMIMBr). Using AFMC, the analytes were prepared in BMIMBr micellar matrix and hydrodynamically injected into the phosphate buffer without IL micelles. The conductivity ratio between BGE and sample (γ, BGE/sample) was optimized to be 3.0 in sweeping-MEKC and 0.33 in AFMC resulting the adequate separation of analytes within 4.0 min. To reduce the possibility of BMIMBr adsorption, an appropriate rinsing protocol was used. The limits of detection were calculated as 0.1 ng/mL MTX, 0.05 ng/mL FNA and 0.05 ng/mL FA by sweeping-MEKC and 0.5 ng/mL MTX, 0.3 ng/mL FNA and 0.3 ng/mL FA by AFMC. The accuracy was tested by recovery in plasma and urine matrices giving values ranging between 90 and 110%. Both stacking and sweeping by BMIMBr could be successfully used for the rapid, selective and sensitive determination of pharmaceuticals in complex matrices due to its fascinating properties, including high conductivity, good thermal stability and ability to form different types of interactions by electrostatic, hydrophobic, hydrogen bonding and π-π interactions. In sweeping-MEKC, the using of BMIMBr enhanced the γ factor, k retention factor and the injected amount of sample. Consequently, this technique offers particular potential for higher sensitivity by giving 22- and 5-fold sensitivity enhancement factors (SEFs) of MTX compared to CZE and AFMC, respectively. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim. Source

Mozafari M.,Institute of Medicinal and Pharmaceutical Chemistry | Nachbar M.,Institute of Medicinal and Pharmaceutical Chemistry | El Deeb S.,Institute of Medicinal and Pharmaceutical Chemistry

CE is one of the most important analytical techniques. Although the injected sample volume in CE is only in the nanoliter range, most commercial CE instruments need approximately 50 μL of the sample in the injection vial to perform the analysis. Hence, in order to fully profit from the low injection volumes, smaller vial volumes are required. Thus experiments were performed using silicone oil, which has higher density than water (1.09 g/mL) to replace sample dead volume in the vial. The results were compared to those performed without using the silicone oil in the sample vial. As an example five standard proteins namely beta-lactoglobulin, BSA, HSA, myoglobin, and ovalbumin, and one of the coagulation cascade involved proteins called vitonectin were investigated using CE. Mobility ratios and peak areas were compared. However, no significant changes were observed (RSDs% for mobility ratios and peak areas were better than 0.9 and 5.8%, respectively). Afterwards, an affinity CE method was used to investigate the interactions of two proteins, namely HSA and vitronectin, with three ligands namely enoxaparin sodium, unfractionated heparin, and pentosan polysulfate sodium. Mobility shift precision results showed that the employment of the filling has no noticeable effect on any of the protein-ligand interactions. Using a commercial PrinCE instrument and an autosampler the required sample volume is reduced down to 10 μL, and almost this complete volume can be subsequently injected during repeated experiments. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim. Source

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